CN114411130A - Thick electroless copper plating solution with good ductility - Google Patents
Thick electroless copper plating solution with good ductility Download PDFInfo
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- CN114411130A CN114411130A CN202111633302.9A CN202111633302A CN114411130A CN 114411130 A CN114411130 A CN 114411130A CN 202111633302 A CN202111633302 A CN 202111633302A CN 114411130 A CN114411130 A CN 114411130A
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- copper plating
- plating solution
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
- C23C18/405—Formaldehyde
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
- H05K3/42—Plated through-holes or plated via connections
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- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- General Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
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- Chemically Coating (AREA)
Abstract
The invention provides a thick chemical copper plating solution with good ductility, which is formed by mixing chemical copper plating solution A, chemical copper plating solution B, chemical copper plating solution M and deionized water; the chemical copper plating solution A comprises 160-220g/L soluble copper salt and 80-160g/L reducing agent, the chemical copper plating solution B comprises 180-220g/L sodium hydroxide, 30-60ml/L methanol, 20-60g/L complexing agent and 0.1-0.5g/L stabilizing agent, and the chemical copper plating solution M comprises 1-2g/L stabilizing agent, 2-5g/L plasticizer, 1-3g/L wetting agent and 200-400g/L complexing agent. The electroless copper plating solution disclosed by the invention has the advantages that the deposition rate is ensured, meanwhile, the brittleness of an electroless copper plating layer is reduced, an electroless copper plating deposition layer with good ductility is obtained, the prepared electroless copper plating film has good ductility and bending resistance, and the reliability of PCB hole metallization is further improved.
Description
Technical Field
The invention relates to the technical field of circuit board copper plating, in particular to a thick chemical copper plating solution with good ductility.
Background
Electroless plating is a metal deposition process in which metal ions are reduced by the autocatalytic action of the metal surface by means of a suitable reducing agent in solution, and electroless plating can only be carried out on catalytically active surfaces.
The traditional non-metal surface activation method adopts colloid palladium, but the colloid stability is poor, and the palladium price is high, so that the activation cost is high. Thus, low palladium processes are emerging.
The chemical copper plating solution mainly comprises copper salt, a reducing agent, a complexing agent, a stabilizing agent, a pH value regulator and other additives. Formaldehyde is used as a reducing agent in most commercial chemical copper plating solutions, two basic chemical reactions exist in the reaction process, namely, copper ions obtain electrons and are changed into copper simple substances, and the formaldehyde reacts with hydroxyl ions to produce hydrogen and water and carboxylic acid ions and give out electrons; besides the effective oxidation-reduction reaction of copper ions on the catalytic surface, which is reduced into metallic copper by formaldehyde, a plurality of side reactions mainly comprise the Cannizzaro reaction and the non-catalytic reaction, in the non-catalytic reaction, cuprous oxide particles are reduced out, and then cuprous oxide can be reduced into particle copper by further reaction, the side reactions not only consume the effective components in the particles, but also generate cuprous oxide, copper and superfine powder which are suspended in the plating solution and are difficult to be removed by a filtering method, so that the plating solution is easy to decompose, if the cuprous oxide and the copper are co-deposited, the copper deposition layer is loosened and rough on the surface of the piece to be plated, so that the copper deposition layer, namely the copper plating layer has poor binding force with the base body of the piece to be plated, and the copper plating solution can be further damaged due to the increase of the copper powder.
One of the most important fields of application of electroless copper plating in industry at present is the process of metallizing through holes of printed circuit boards, wherein a layer of copper is deposited in the wall of an insulating hole of a printed circuit board to metallize the through hole, so that the plated layer is electroplated and thickened to conduct circuits between layers.
The PCB chemical copper plating process can divide chemical copper plating into a thin copper system and a thick copper system according to different thicknesses of plating layers, the thick copper process is adopted without full-plate electroplating thickening, the production flow can be shortened, the cost is reduced, and some PCB manufacturers are widely used. The ductility of the electroless copper plating is much lower than that of the electrolytic copper plating, the conventional electroless copper plating layer is generally very thin (0.3-0.5 microns) and can meet the reliability requirement of PCB hole metallization, but the thick copper plating process generally deposits the thickness of 1-2 microns and puts higher requirements on the physical performance of the electroless copper plating, the plating speed is faster, the plating layer is required to have certain ductility, and the thermal expansion, fracture and delamination of the PCB at the rear under the condition of subsequent reflow soldering high-temperature treatment are ensured.
Therefore, there is still a need to improve the physical properties of thick copper process coatings, such as ductility, and to improve the quality of via metallization.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a thick electroless copper plating solution with good ductility.
The technical scheme of the invention is as follows: the thick electroless copper plating solution with good ductility is formed by mixing electroless copper plating solution A, electroless copper plating solution B, electroless copper plating solution M and deionized water;
wherein the electroless copper plating solution A comprises the following components in concentration: 160-220g/L soluble copper salt and 80-160g/L reducing agent, wherein the concentration is the concentration of each component in the electroless copper plating solution A;
the electroless copper plating B solution comprises the following components in concentration: 180-220g/L sodium hydroxide, 30-60ml/L methanol, 20-60g/L complexing agent and 0.1-0.5g/L stabilizing agent, wherein the concentration is the concentration of each component in the chemical copper plating solution B;
the electroless copper plating M solution comprises the following components in concentration: 1-2g/L stabilizer, 2-5g/L plasticizer, 1-3g/L wetting agent and 200-400g/L complexing agent, wherein the concentration is the concentration of each component in the electroless copper plating M solution.
Preferably, the concentration of the soluble copper salt in the electroless copper plating solution A is 180-200 g/L.
Preferably, the soluble copper salt is copper sulfate pentahydrate.
Preferably, the concentration of the sodium hydroxide in the electroless copper plating B solution is 190-210 g/L.
Preferably, the concentration of the complexing agent in the electroless copper plating solution B is 30-50 g/L.
Preferably, the reducing agent in the electroless copper plating solution A is formaldehyde.
Preferably, the complexing agent in the electroless copper plating solution B and the electroless copper plating solution M is selected from the following groups: tartaric acid, ethylenediamine tetraacetic acid, ethylenediamine tetrapropionic acid, triethanolamine, nitrilotriacetic acid, and dimethylol ethylenediamine tetraacetic acid.
Preferably, the stabilizing agent in the electroless copper plating solution B and the electroless copper plating solution M is selected from the following components: 4, 4-bipyridine, mercaptobenzothiazole, potassium ferrocyanide and potassium thiocyanate.
Preferably, the electroless copper plating plasticizer is selected from the group consisting of: one or two or more of tetraisopropoxytitanium, polybutyl titanate, tetraisopropoxytitanium and isopropyl stearate.
Preferably, the wetting agent is selected from at least one of polyethylene oxide and a surfactant FC-4430.
Preferably, the volume ratio of the electroless copper plating solution A, the electroless copper plating solution B, the electroless copper plating solution M and the deionized water in the electroless copper plating mixed solution is 5:7:10: 78.
Preferably, the invention also provides a method for plating copper on a PCB by using the electroless copper plating mixed solution, which comprises the following steps:
s1), pre-treating the PCB, sequentially carrying out bulking, washing, removing glue residues, recycling and washing, pre-neutralizing, washing, pore-finishing, washing, micro-etching, washing, pre-dipping, activating, washing, accelerating and washing on the PCB to obtain the PCB with the surface completely exposed with the metal palladium;
s2) chemically plating copper on the substrate, adding a chemical copper plating solution into a reaction tank, maintaining the temperature of the solution at 30-40 ℃, immersing the substrate pretreated in the step S1) into the chemical copper plating solution, catalyzing the chemical copper plating reaction through the activation of metal palladium, and chemically plating copper on the substrate and the copper surface of the hole for 25-35min, wherein the chemical copper plating thickness on the substrate surface is 1-2 microns.
The invention has the beneficial effects that:
1. the electroless copper plating film prepared by the electroless copper plating solution has good ductility and bending resistance, so that the reliability of PCB hole metallization is improved;
2. the electroless copper plating solution disclosed by the invention can reduce the brittleness of an electroless copper plating layer while ensuring the deposition rate, obtain an electroless copper plating deposition layer with good ductility and increase the reliability of PCB hole metallization.
Detailed Description
The following further illustrates embodiments of the invention:
example 1
The embodiment provides a thick electroless copper plating solution with good ductility, which consists of an electroless copper plating solution A, an electroless copper plating solution B, an electroless copper plating solution M and deionized water;
in this embodiment, the volume of each component in the thick electroless copper plating solution is:
wherein the electroless copper plating solution A comprises 160g/L of blue copperas, 80g/L of formaldehyde and the balance of pure water;
the electroless copper plating solution B comprises 180g/L of sodium hydroxide, 40g/L of dihydroxymethyl ethylenediamine tetraacetic acid, 0.1g/L of 4,4' -bipyridyl, 0.5g/L of potassium thiocyanate, 30ml/L of methanol and the balance of pure water;
the electroless copper plating M solution comprises 2g/L potassium thiocyanate, 3g/L isopropyl stearate, 1.5g/L polyethylene oxide (molecular weight 100,000), 300g/L ethylene diamine tetraacetic acid and the balance of pure water.
In this embodiment, the working temperature of the electroless copper plating solution is 35 ℃.
Example 2
The embodiment provides a thick electroless copper plating solution with good ductility, which consists of electroless copper plating solution A, electroless copper plating solution B, electroless copper plating solution M and deionized water.
In this embodiment, the volume of each component in the thick electroless copper plating solution is:
in this embodiment, the working temperature of the electroless copper plating solution is 40 ℃.
Wherein the electroless copper plating solution A comprises 180g/L of blue vitriol, 120g/L of formaldehyde and the balance of pure water;
the electroless copper plating solution B comprises 200g/L of sodium hydroxide, 60g/L of ethylene diamine tetraacetic acid, 0.1g/L of 4,4' -bipyridyl, 0.4g/L of potassium ferrocyanide, 60ml/L of methanol and the balance of pure water;
the electroless copper plating solution M comprises 1g/L potassium ferrocyanide, 5g/L titanium tetraisopropoxide, 1g/L polyethylene oxide (molecular weight 100,000), 400g/L tartaric acid and the balance of pure water.
Example 3
The embodiment provides a thick electroless copper plating solution with good ductility, which consists of electroless copper plating solution A, electroless copper plating solution B, electroless copper plating solution M and deionized water.
In this embodiment, the volume of each component in the thick electroless copper plating solution is:
the working temperature of the electroless copper plating solution is 38 ℃.
Wherein the electroless copper plating solution A comprises 220g/L of blue copperas, 90g/L of formaldehyde and the balance of pure water;
the chemical copper plating solution B comprises 220g/L of sodium hydroxide, 40g/L of triethanolamine, 0.2g/L of 4,4' -bipyridyl, 0.5g/L of potassium ferrocyanide, 40ml/L of methanol and the balance of pure water;
the electroless copper plating solution M comprises 2g/L potassium ferrocyanide, 1g/L titanium tetraisopropoxide, 3g/L surfactant FC-4430, 200g/L ethylene diamine tetraacetic acid and the balance of pure water.
Example 4
The embodiment provides a thick electroless copper plating solution with good ductility, which consists of electroless copper plating solution A, electroless copper plating solution B, electroless copper plating solution M and deionized water.
In this embodiment, the volume of each component in the thick electroless copper plating solution is:
the working temperature of the electroless copper plating solution is 45 ℃.
Wherein the electroless copper plating solution A comprises 190g/L of blue vitriol, 90g/L of formaldehyde and the balance of pure water;
the electroless copper plating solution B comprises 190g/L of sodium hydroxide, 50g/L of ethylene diamine tetraacetic acid, 0.2g/L of 4,4' -bipyridyl, 0.3g/L of potassium ferrocyanide, 60ml/L of methanol and the balance of pure water;
the electroless copper plating M solution comprises 1.8g/L potassium ferrocyanide, 1g/L titanium tetraisopropoxide, 1.5g/L surfactant FC-4430, 200g/L tartaric acid and the balance of pure water.
Example 5
The embodiment provides a thick electroless copper plating solution with good ductility, which consists of electroless copper plating solution A, electroless copper plating solution B, electroless copper plating solution M and deionized water.
In this embodiment, the volume of each component in the thick electroless copper plating solution is:
the working temperature of the electroless copper plating solution is 38 ℃.
Wherein the electroless copper plating solution A comprises 210g/L of blue copperas, 90g/L of formaldehyde and the balance of pure water;
the chemical copper plating solution B comprises 180g/L of sodium hydroxide, 50g/L of tartaric acid, 0.1g/L of 4,4' -bipyridyl, 0.45g/L of potassium ferrocyanide, 40ml/L of methanol and the balance of pure water;
the electroless copper plating M solution comprises 1.6g/L potassium ferrocyanide, 1.2g/L isopropyl stearate, 1.2g/L surfactant polyethylene oxide (molecular weight 100,000), 350g/L ethylene diamine tetraacetic acid and the balance of pure water.
Comparative example 1
The electroless copper plating solution A comprises 160g/L of blue vitriol, 80g/L of formaldehyde and the balance of pure water; the electroless copper plating solution B comprises 180g/L of sodium hydroxide, 40g/L of dihydroxymethyl ethylenediamine tetraacetic acid, 0.1g/L of 2,2' -bipyridyl, 0.5g/L of potassium thiocyanate, 30ml/L of methanol and the balance of pure water; the electroless copper plating M solution comprises 2g/L potassium thiocyanate, 300g/L ethylene diamine tetraacetic acid and the balance of pure water.
Example 6
The electroless copper plating solutions of examples 1 to 5 and comparative example 1 were prepared in the same amounts, and the same-quality and same-size PCB and resin board were subjected to electroless copper plating treatment using the prepared solutions for 30 minutes.
And after the electroless copper plating is finished, taking out the PCB for backlight test, appearance test and deposition thickness test. The experimental procedure of the resin sheet using SEM backlight is as follows:
1. cutting off the reserved slicing holes on the plate, and grinding the taken slices to the central line of a row of holes by using a grinder;
2. grinding with a grinder to a slice thickness of less than 1/8 inches;
3. the slice is placed on the light source of a magnifier, and the coverage of the settled layer in the hole is observed under the magnifier of 10-50 times. The elongation is the ratio of the elongation after the sample is pulled off to the original sample length, and is measured by a ductility tester, and the experimental results are shown in table 1.
Table 1 test comparison results of electroless copper plating solutions of examples 1 to 5 and comparative example 1.
From the above experimental results, it can be seen that the electroless copper plating solution of the present invention has a high deposition rate, further improves the ductility of the plating layer, and has a high reliability of hole metallization.
The foregoing embodiments and description have been presented only to illustrate the principles and preferred embodiments of the invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention as hereinafter claimed.
Claims (10)
1. The thick electroless copper plating solution with good ductility is characterized by being prepared by mixing electroless copper plating solution A, electroless copper plating solution B, electroless copper plating solution M and deionized water;
wherein the volume ratio of the electroless copper plating solution A, the electroless copper plating solution B, the electroless copper plating solution M to the deionized water is 5:7:10: 78;
wherein the electroless copper plating solution A comprises the following components in concentration: 160-220g/L soluble copper salt and 80-160g/L reducing agent, wherein the concentration is the concentration of each component in the electroless copper plating solution A;
the electroless copper plating B solution comprises the following components in concentration: 180-220g/L sodium hydroxide, 30-60ml/L methanol, 20-60g/L complexing agent and 0.1-0.5g/L stabilizing agent, wherein the concentration is the concentration of each component in the chemical copper plating solution B;
the electroless copper plating M solution comprises the following components in concentration: 1-2g/L stabilizer, 2-5g/L plasticizer, 1-3g/L wetting agent and 200-400g/L complexing agent, wherein the concentration is the concentration of each component in the electroless copper plating M solution.
2. A thick electroless copper plating solution with good ductility according to claim 1, wherein: the concentration of the soluble copper salt in the electroless copper plating solution A is 180-200 g/L.
3. A thick electroless copper plating solution with good ductility according to claim 1, wherein: the soluble copper salt is copper sulfate pentahydrate; the reducing agent in the electroless copper plating solution A is formaldehyde.
4. A thick electroless copper plating solution with good ductility according to claim 1, wherein: the concentration of the sodium hydroxide in the electroless copper plating B solution is 190-210 g/L.
5. A thick electroless copper plating solution with good ductility according to claim 1, wherein: the concentration of the complexing agent in the chemical copper plating solution B is 30-50 g/L.
6. A thick electroless copper plating solution with good ductility according to claim 1, wherein: the complexing agents in the chemical copper plating solution B and the chemical copper plating solution M are respectively selected from two or more than two of tartaric acid, ethylene diamine tetraacetic acid, ethylene diamine tetrapropionic acid, triethanolamine, nitrilotriacetic acid and dimethylol ethylene diamine tetraacetic acid.
7. A thick electroless copper plating solution with good ductility according to claim 1, wherein: and the stabilizing agent in the chemical copper plating solution B and the chemical copper plating solution M is selected from at least one of 4, 4-bipyridyl, mercaptobenzothiazole, potassium ferrocyanide and potassium thiocyanate.
8. A thick electroless copper plating solution with good ductility according to claim 1, wherein: the plasticizer for electroless copper plating is one or two or more selected from titanium tetraisopropoxide, polybutyl titanate, titanium tetraisopropoxide and isopropyl tristearate.
9. A thick electroless copper plating solution with good ductility according to claim 1, wherein: the wetting agent is selected from at least one of polyethylene oxide and a surfactant FC-4430.
10. A method for copper plating of PCB boards using an electroless copper plating solution according to any of claims 1 to 9, comprising the steps of:
s1), pre-treating the PCB, sequentially carrying out bulking, washing, removing glue residues, recycling and washing, pre-neutralizing, washing, pore-finishing, washing, micro-etching, washing, pre-dipping, activating, washing, accelerating and washing on the PCB to obtain the PCB with the surface completely exposed with the metal palladium;
s2) electroless copper plating of the substrate, adding the electroless copper plating solution according to any one of claims 1 to 9 into a reaction tank, maintaining the temperature of the solution at 30 to 40 ℃, then immersing the substrate pretreated in the step S1) into the electroless copper plating solution, catalyzing the electroless copper plating reaction through the activation of metallic palladium, and electroless copper plating on the substrate and the copper surface of the hole, wherein the reaction time is 25 to 35min, and the surface of the substrate is plated with copper with the thickness of 1 to 2 microns.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111633302.9A CN114411130A (en) | 2021-12-29 | 2021-12-29 | Thick electroless copper plating solution with good ductility |
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| CN202111633302.9A CN114411130A (en) | 2021-12-29 | 2021-12-29 | Thick electroless copper plating solution with good ductility |
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| CN106413289A (en) * | 2016-11-21 | 2017-02-15 | 奥士康精密电路（惠州）有限公司 | Copper deposition method for preventing occurrence of copper-free hole |
| CN110512199A (en) * | 2019-09-26 | 2019-11-29 | 苏州天承化工有限公司 | A kind of chemical bronze plating liquid and preparation method thereof |
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2021
- 2021-12-29 CN CN202111633302.9A patent/CN114411130A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104152875A (en) * | 2014-08-25 | 2014-11-19 | 志超科技（遂宁）有限公司 | PCB-PTH (Printed Circuit Board-Plated Through Hole) line hole conditioning and activation ultrasonic device and method |
| CN104651814A (en) * | 2014-11-28 | 2015-05-27 | 广东致卓精密金属科技有限公司 | Chemical copper plating solution and chemical copper plating method |
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